CN102382548A - Solvent-free epoxy coating for inner wall of petroleum storage tank and preparation method - Google Patents
Solvent-free epoxy coating for inner wall of petroleum storage tank and preparation method Download PDFInfo
- Publication number
- CN102382548A CN102382548A CN2011102485728A CN201110248572A CN102382548A CN 102382548 A CN102382548 A CN 102382548A CN 2011102485728 A CN2011102485728 A CN 2011102485728A CN 201110248572 A CN201110248572 A CN 201110248572A CN 102382548 A CN102382548 A CN 102382548A
- Authority
- CN
- China
- Prior art keywords
- liquid
- coating
- storage tank
- order
- proportion
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Paints Or Removers (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to a solvent-free epoxy coating for the inner wall of a petroleum storage tank and a preparation method. Solution A comprises E-51 epoxy resin, butyl glycidyl ether, KH-560 silane coupling agent, ALCOPHOR827 anti-corrosion auxiliary agent, BYK-085 flatting agent, Efka-722 defoamer, 400 mesh rutile type titanium white, 325 mesh baryte powder, 400 mesh talcum powder, carbon black and 881-B organic bentonite. Solution B comprises polyamide EU8235 epoxy hardener, dimethylbenzene and normal butanol. The weight percent of the solution A is 80% to 90%. The solvent-free epoxy coating is safe and environment friendly, the coating volume shrinkage is 1.15% to 1.5%, the pull-off adhesion is 16.5MPa to 20.0MPa, a chemical media resistance 90d paint film is in good condition, and a salt spray resistance 3000h paint film is in good condition. With the adoption of the solvent-free epoxy coating, corrosion of the storage tank can be greatly reduced, and the service life of the storage tank can be greatly prolonged.
Description
Technical field
The present invention relates to a kind of solventless epoxy coating and method of manufacture, be applicable to the inner wall anti-corrosive of petroleum storage tank.
Background technology
Existing petroleum storage tank inner wall anti-corrosive adopts solvent-borne type anticorrosive coating (volumetric shrinkage is 2%~3%) more, and its weak point is that the volatilization of solvent makes coating occur defectives such as pin hole easily on the one hand, and coating antiseptic erosion performance can't effectively be guaranteed; Can cause the environmental pollution and the wasting of resources on the other hand, and poison bigger operating personnel's health; Exist when under the storage tank closed environment, constructing in addition and dodge quick-fried danger.
Summary of the invention
The purpose of this invention is to provide a kind of solventless epoxy coating and method of manufacture.Coating has good application property and Safety and Environmental Protection, and coating has smaller volume shrinking percentage and good corrosion prevention performance.Guarantee the work-ing life of storage tank, solve the safety and environmental protection problem of solvent-borne type anticorrosive coating.
The technical scheme that the present invention adopts is:
One, the raw material of solventless epoxy coating and prescription
Raw material comprises:
1, E-51 epoxy resin
The chief editor of coating process editorial committee, coating process (third edition) first volume, Chemical Industry Press, 1997, the 631 pages.
Character: transparent liquid, do not have obvious mechanical impurity, oxirane value 0.48~0.54eq/100g.
Purposes: be used as film-forming resin.
Factory: Jiangsu three wood
2, butylglycidyl ether
The chief editor of coating process editorial committee, coating process (third edition) first volume, Chemical Industry Press, 1997, the 682 pages.
Character: colourless transparent liquid, oxirane value 0.65eq/100g.
Purposes: reduce dope viscosity.
Factory: the prosperous Dehua worker in Yueyang.
3, KH-560 silane coupling agent
The Guo Shujing chief editor, domestic and international coatings additive(s) kind handbook, Chemical Industry Press, 1999, the 6 pages.
Character: light yellow liquid, specific density 1.065~1.069.
Purposes: coupling is built bridge, and improves paint machine performance, bonding ability, water resistance.
Factory: chemical plant, Gaizhou City.
4, ALCOPHOR827 protection against corrosion auxiliary agent
The Guo Shujing chief editor, domestic and international coatings additive(s) kind handbook, Chemical Industry Press, 1999, the 368 pages.
Character: white powder, bulk density 135~150g/L, particle diameter<16 μ m.
Purposes: improve the coating antiseptic performance.
Factory: Henkel Corp..
5, BYK-085 flow agent
The Guo Shujing chief editor, domestic and international coatings additive(s) kind handbook, Chemical Industry Press, 1999, the 605 pages.
Character: methyl alkyl ZGK 5, density (20 ℃) 0.91g/cm
3
Purposes: levelling.
Factory: German Bi Ke chemical company.
6, Efka-722 skimmer
The Guo Shujing chief editor, domestic and international coatings additive(s) kind handbook, Chemical Industry Press, 1999, the 152 pages.
Character: acetate methoxyl group propyl ester/korenyl.
Purposes: froth breaking.
Factory: Dutch EFKA auxiliary agent company.
7, Rutile type Titanium Dioxide (400 order)
The chief editor of coating process editorial committee, coating process (third edition) first volume, Chemical Industry Press, 1997, the 30 pages.
Character: specific refractory power 2.74, specific density 4.2~4.3.
Purposes: white pigment.
Factory: Nanjing Titanium Dioxide Chemical Co., Ltd..
8, ground barium sulfate (325 order)
The chief editor of coating process editorial committee, coating process (third edition) first volume, Chemical Industry Press, 1997, the 50 pages.
Character: fine and close white powder, density 4.3~4.5g/cm
3
Purposes: improve the paint flow levelling, increase hardness of paint film and wear resistance.
Factory: Yidu City Austria reaches chemical industry ltd.
9, talcum powder (400 order)
The chief editor of coating process editorial committee, coating process (third edition) first volume, Chemical Industry Press, 1997, the 49 pages.
10, carbon black
The chief editor of coating process editorial committee, coating process (third edition) first volume, Chemical Industry Press, 1997, the 32 pages.
11,881-B organobentonite
The chief editor of coating process editorial committee, coating process (third edition) first volume, Chemical Industry Press, 1997, the 137 pages.
12, polymeric amide EU8235 epoxy hardener
The chief editor of coating process editorial committee, coating process (third edition) first volume, Chemical Industry Press, 1997, the 646 pages.
Purposes: solidifying agent.
Factory: the female Industrial Co., Ltd. of Shanghai moral.
13, YLENE (technical pure)
14, propyl carbinol (technical pure)
Each weight percentages of components of solventless epoxy coating is:
1, A liquid (each weight percentages of components sum is 100%):
1) E-51 epoxy resin: 45~55%;
2) butylglycidyl ether: 5~10%;
3) KH-560 silane coupling agent: 0.25~0.4%;
4) ALCOPHOR827 protection against corrosion auxiliary agent: 0.8~1.5%;
5) BYK-085 flow agent: 0.04~0.3%;
6) Efka-722 skimmer: 0.4~1.2%;
7) Rutile type Titanium Dioxide (400 order): 5~10%;
8) ground barium sulfate (325 order): 15~20%;
9) talcum powder (400 order): 15~20%;
10) carbon black: 0.1~0.5%;
11) 881-B organobentonite: 0.1~1%.
2, B liquid (each weight percentages of components sum is 100%):
1) polymeric amide EU8235 epoxy hardener: 75~85%;
2) YLENE: 10~15%;
3) propyl carbinol: 5~10%.
During use, A liquid and B liquid are mixed coating, wherein the weight percent of A liquid in coating is: 80~90%.
Two, the preparation method of solventless epoxy coating
Major equipment:
Impeller, sand mill.
Working method:
Add E-51 epoxy resin and butylglycidyl ether in the container in proportion; Mix; Under agitation add KH-560 silane coupling agent, ALCOPHOR827 protection against corrosion auxiliary agent, BYK-085 flow agent, Efka-722 skimmer then successively in proportion; Mix; Then under agitation add Rutile type Titanium Dioxide (400 order) successively in proportion, ground barium sulfate (325 order), talcum powder (400 order), carbon black, 881-B organobentonite are promptly processed the A liquid in this coating with grinding 0.5h with sand mill behind the impeller high-speed stirring 0.5h; Polymeric amide EU8235 epoxy hardener, YLENE and propyl carbinol are added in another container in proportion, mix the B liquid of promptly processing in this coating with impeller.
Three, the method for use of solventless epoxy coating
During use, A and B liquid are mixed in proportion and stirs, process solventless epoxy coating, in 30 minutes, workpiece is carried out the airless spraying construction.
Beneficial effect of the present invention
Coating has good application property and Safety and Environmental Protection.Coating volumetric shrinkage 1.15%~1.50% draws back method sticking power 16.5MPa~20.0MPa, resistant to chemical media property (10%H
2SO
4, 10%NaOH, 10%NaCl solution, normal temperature) the 90d paint film is intact, salt spray resistance 3000h paint film is intact.The inner wall anti-corrosive that can be used for crude oil, sewage storage tank can reduce the storage tank corrosion, the work-ing life of improving storage tank significantly.
Embodiment
Embodiment 1: solventless epoxy coating, and each weight percentages of components is:
A liquid:
E-51 epoxy resin: 51.5%;
Butylglycidyl ether: 5.5%;
KH-560 silane coupling agent 0.28%;
ALCOPHOR827 protection against corrosion auxiliary agent 0.9%;
BYK-085 flow agent 0.08%;
Efka-722 skimmer 0.6%;
Rutile type Titanium Dioxide (400 order): 7.5%;
Ground barium sulfate (325 order): 16.5%;
Talcum powder (400 order): 16.5%;
Carbon black: 0.50%;
881-B organobentonite: 0.14%.
B liquid:
Polymeric amide EU8235 epoxy hardener: 81%;
YLENE: 12%;
Propyl carbinol: 7%.
The weight percent of A liquid in coating is 82%.
The preparation method is:
Add E-51 epoxy resin and butylglycidyl ether in the container in proportion; Mix; Under agitation add KH-560 silane coupling agent, ALCOPHOR827 protection against corrosion auxiliary agent, BYK-085 flow agent, Efka-722 skimmer then successively in proportion; Mix; Then under agitation add Rutile type Titanium Dioxide (400 order) successively in proportion, ground barium sulfate (325 order), talcum powder (400 order), carbon black, 881-B organobentonite are promptly processed the A liquid in this coating with grinding 0.5h with sand mill behind the impeller high-speed stirring 0.5h; Polymeric amide EU8235 epoxy hardener, YLENE and propyl carbinol are added in another container in proportion, mix the B liquid of promptly processing in this coating with impeller.During use, A and B liquid mixed in proportion process solventless epoxy coating, solidify to form coating through normal temperature.
Effect: coating volumetric shrinkage 1.18%, draw back method sticking power 18.4MPa, resistant to chemical media property (10%H
2SO
4, 10%NaOH, 10%NaCl solution, normal temperature) the 90d paint film is intact, salt spray resistance 3000h paint film is intact.
Embodiment 2: solventless epoxy coating, and each weight percentages of components is:
A liquid:
E-51 epoxy resin: 53.5%;
Butylglycidyl ether: 5.6%;
KH-560 silane coupling agent 0.32%;
ALCOPHOR827 protection against corrosion auxiliary agent 1.1%;
BYK-085 flow agent 0.1%;
Efka-722 skimmer 0.5%;
Rutile type Titanium Dioxide (400 order): 6%;
Ground barium sulfate (325 order): 16%;
Talcum powder (400 order): 16%;
Carbon black: 0.28%;
881-B organobentonite: 0.6%.
B liquid:
Polymeric amide EU8235 epoxy hardener: 80%;
YLENE: 13.5%;
Propyl carbinol: 6.5%.
The weight percent of A liquid in coating is 84%.
The preparation method of embodiment 2 solventless epoxy coatings is identical with embodiment 1.
Effect: coating volumetric shrinkage 1.22%, draw back method sticking power 17.9MPa, resistant to chemical media property (10%H
2SO
4, 10%NaOH, 10%NaCl solution, normal temperature) the 90d paint film is intact, salt spray resistance 3000h paint film is intact.
Embodiment 3: solventless epoxy coating, and each weight percentages of components is:
A liquid:
E-51 epoxy resin: 47.5%;
Butylglycidyl ether: 6.5%;
KH-560 silane coupling agent 0.34%;
ALCOPHOR827 protection against corrosion auxiliary agent 1.2%;
BYK-085 flow agent 0.16%;
Efka-722 skimmer 0.9%;
Rutile type Titanium Dioxide (400 order): 8%;
Ground barium sulfate (325 order): 16.5%;
Talcum powder (400 order): 18%;
Carbon black: 0.2%;
881-B organobentonite: 0.7%.
B liquid:
Polymeric amide EU8235 epoxy hardener: 83%;
YLENE: 11.5%;
Propyl carbinol: 5.5%.
The weight percent of A liquid in coating is 81%.
The preparation method of embodiment 3 solventless epoxy coatings is identical with embodiment 1.
Effect: coating volumetric shrinkage 1.14%, draw back method sticking power 19.8MPa, resistant to chemical media property (10%H
2SO
4, 10%NaOH, 10%NaCl solution, normal temperature) the 90d paint film is intact, salt spray resistance 3000h paint film is intact.
Embodiment 4: solventless epoxy coating, and each weight percentages of components is:
A liquid:
E-51 epoxy resin: 53%;
Butylglycidyl ether: 5.5%;
KH-560 silane coupling agent 0.3%;
ALCOPHOR827 protection against corrosion auxiliary agent 1.4%;
BYK-085 flow agent 0.2%;
Efka-722 skimmer 1.1%;
Rutile type Titanium Dioxide (400 order): 5.5%;
Ground barium sulfate (325 order): 16%;
Talcum powder (400 order): 16%;
Carbon black: 0.3%;
881-B organobentonite: 0.7%.
B liquid:
Polymeric amide EU8235 epoxy hardener: 84.5%;
YLENE: 10.5%;
Propyl carbinol: 5%.
The weight percent of A liquid in coating is 88%.
The preparation method of embodiment 4 solventless epoxy coatings is identical with embodiment 1.
Effect: coating volumetric shrinkage 1.26%, draw back method sticking power 17.0MPa, resistant to chemical media property (10%H
28O
4, 10%NaOH, 10%NaCl solution, normal temperature) the 90d paint film is intact, salt spray resistance 3000h paint film is intact.
Claims (2)
1. a petroleum storage tank inwall is used solventless epoxy coating, it is characterized in that forming by A liquid and B liquid, wherein:
Each weight percentages of components is in the A liquid:
E-51 epoxy resin 45~55%;
Butylglycidyl ether 5~10%;
KH-560 silane coupling agent 0.25~0.4%;
ALCOPHOR827 protection against corrosion auxiliary agent 0.8~1.5%;
BYK-085 flow agent 0.04~0.3%;
Efka-722 skimmer 0.4~1.2%;
400 order Rutile type Titanium Dioxides 5~10%;
325 order ground barium sulfates 15~20%;
400 order talcum powder 15~20%;
Carbon black 0.1~0.5%;
881-B organobentonite 0.1~1%;
Each weight percentages of components sum is 100% in the A liquid;
Each weight percentages of components is in the B liquid:
Polymeric amide EU8235 epoxy hardener 75~85%;
YLENE 10~15%;
Propyl carbinol 5~10%;
Each weight percentages of components sum is 100% in the B liquid;
During use, A liquid and B liquid are mixed coating, the weight percent of A liquid in coating is 80~90%, solidify to form coating through normal temperature.
2. the described petroleum storage tank inwall of claim 1 is used the solventless epoxy coating method of manufacture, it is characterized in that:
Add E-51 epoxy resin and butylglycidyl ether in the container in proportion; Mix; Under agitation add KH-560 silane coupling agent, ALCOPHOR827 protection against corrosion auxiliary agent, BYK-085 flow agent, Efka-722 skimmer then successively in proportion; Mix; Then under agitation add 400 order Rutile type Titanium Dioxides successively in proportion, 325 order ground barium sulfates, 400 order talcum powder, carbon black, 881-B organobentonite are promptly processed the A liquid in this coating with grinding 0.5h with sand mill behind the impeller high-speed stirring 0.5h; Polymeric amide EU8235 epoxy hardener, YLENE and propyl carbinol are added in another container in proportion, mix the B liquid of promptly processing in this coating with impeller; During use, A and B liquid mixed in proportion process solventless epoxy coating.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN 201110248572 CN102382548B (en) | 2011-08-26 | 2011-08-26 | Solvent-free epoxy coating for inner wall of petroleum storage tank and preparation method |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN 201110248572 CN102382548B (en) | 2011-08-26 | 2011-08-26 | Solvent-free epoxy coating for inner wall of petroleum storage tank and preparation method |
Publications (2)
Publication Number | Publication Date |
---|---|
CN102382548A true CN102382548A (en) | 2012-03-21 |
CN102382548B CN102382548B (en) | 2013-10-23 |
Family
ID=45822407
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN 201110248572 Active CN102382548B (en) | 2011-08-26 | 2011-08-26 | Solvent-free epoxy coating for inner wall of petroleum storage tank and preparation method |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN102382548B (en) |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103756508A (en) * | 2014-01-08 | 2014-04-30 | 上海麦加涂料有限公司 | Method for preparing environment-friendly coating for inner surface of container |
CN103788830A (en) * | 2014-01-20 | 2014-05-14 | 南通华新环保设备工程有限公司 | Acid and alkali resistant coating for stirring equipment and preparation method thereof |
CN104710910A (en) * | 2015-03-27 | 2015-06-17 | 上海灿达建材科技有限公司 | Solvent-free medium coating and manufacturing method thereof |
CN104927565A (en) * | 2015-05-29 | 2015-09-23 | 大禹伟业(北京)国际科技有限公司 | Waterproof solvent-free epoxy resin coating in drinking water project and construction method thereof |
CN105949961A (en) * | 2016-07-07 | 2016-09-21 | 张学健 | Corrosion-resistant coating applied to red wine fermentation tanks |
CN109913081A (en) * | 2017-12-13 | 2019-06-21 | 深圳市百安百科技有限公司 | A kind of solvent-free and high temperature-resistant anticorrosive paint for crude oil storage tank |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5229438A (en) * | 1989-12-01 | 1993-07-20 | Mitsui Petrochemical Industries, Ltd. | Two-component epoxy resin compositions |
CN1492016A (en) * | 2002-10-24 | 2004-04-28 | 张晓广 | Anti-corrosion paint porticularly for petroleum storage tank and equipment |
CN101074338A (en) * | 2006-05-18 | 2007-11-21 | 中国石油天然气集团公司 | Acid-alkali-corrosive-resisting oil-pipe coating and its production |
US20090042036A1 (en) * | 2006-03-09 | 2009-02-12 | Chugoku Marine Paints, Ltd. | High-solid anticorrosive coating composition |
CN101942258A (en) * | 2009-07-08 | 2011-01-12 | 中国石油天然气集团公司 | Solvent-free epoxy paint for steel roasted elbow and preparation method thereof |
-
2011
- 2011-08-26 CN CN 201110248572 patent/CN102382548B/en active Active
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5229438A (en) * | 1989-12-01 | 1993-07-20 | Mitsui Petrochemical Industries, Ltd. | Two-component epoxy resin compositions |
CN1492016A (en) * | 2002-10-24 | 2004-04-28 | 张晓广 | Anti-corrosion paint porticularly for petroleum storage tank and equipment |
US20090042036A1 (en) * | 2006-03-09 | 2009-02-12 | Chugoku Marine Paints, Ltd. | High-solid anticorrosive coating composition |
CN101074338A (en) * | 2006-05-18 | 2007-11-21 | 中国石油天然气集团公司 | Acid-alkali-corrosive-resisting oil-pipe coating and its production |
CN101942258A (en) * | 2009-07-08 | 2011-01-12 | 中国石油天然气集团公司 | Solvent-free epoxy paint for steel roasted elbow and preparation method thereof |
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103756508A (en) * | 2014-01-08 | 2014-04-30 | 上海麦加涂料有限公司 | Method for preparing environment-friendly coating for inner surface of container |
CN103756508B (en) * | 2014-01-08 | 2016-05-04 | 上海麦加涂料有限公司 | A kind of preparation method of the environmental protection coating material for container inner surface |
CN103788830A (en) * | 2014-01-20 | 2014-05-14 | 南通华新环保设备工程有限公司 | Acid and alkali resistant coating for stirring equipment and preparation method thereof |
CN104710910A (en) * | 2015-03-27 | 2015-06-17 | 上海灿达建材科技有限公司 | Solvent-free medium coating and manufacturing method thereof |
CN104927565A (en) * | 2015-05-29 | 2015-09-23 | 大禹伟业(北京)国际科技有限公司 | Waterproof solvent-free epoxy resin coating in drinking water project and construction method thereof |
CN104927565B (en) * | 2015-05-29 | 2017-09-29 | 大禹伟业(北京)国际科技有限公司 | Water proof type solventless epoxy resin coating and its construction method in drinking water project |
CN105949961A (en) * | 2016-07-07 | 2016-09-21 | 张学健 | Corrosion-resistant coating applied to red wine fermentation tanks |
CN109913081A (en) * | 2017-12-13 | 2019-06-21 | 深圳市百安百科技有限公司 | A kind of solvent-free and high temperature-resistant anticorrosive paint for crude oil storage tank |
Also Published As
Publication number | Publication date |
---|---|
CN102382548B (en) | 2013-10-23 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN102382548B (en) | Solvent-free epoxy coating for inner wall of petroleum storage tank and preparation method | |
CN102618159B (en) | Water-based polyurethane anticorrosive coating for containers and preparation method for coating | |
CN102533029B (en) | Aqueous asphalt imitation anticorrosion coating for container chassis and preparation method thereof | |
CN102352168B (en) | Anticorrosive wear-resistant paint for magnesium alloy and preparation method thereof | |
CN102702899B (en) | Water-based modified pure acrylic acid anticorrosive paint | |
CN102816496B (en) | Polyaniline/attapulgite nano-material antirust primer and preparation method thereof | |
CN101294044B (en) | Solvent-free static electricity conductive anticorrosive paint for oil storage tank and production method | |
CN101215438A (en) | Anti-soiling aging-resisting stainless steel paint and preparation method thereof | |
CN103980797A (en) | Polyurethane modified epoxy resin anticorrosive nano-coating | |
CN101993645A (en) | Water-based heavy corrosion protection ceramic paint | |
CN109370364A (en) | It is a kind of for relating to the nano anticorrosive coating and preparation method thereof of metal surface under acid environment | |
CN106221563A (en) | A kind of two component epoxy class anti-corrosive organic coatings and preparation method thereof and using method | |
CN102993859A (en) | Zinc powder-free shop primer and preparation method thereof | |
CN101333404B (en) | Water-soluble epoxy red ferric oxide primer and method of preparing same | |
CN104327650B (en) | The preparation method of methyl silicate water nano antirust agent | |
CN104479501A (en) | Self-cleaning waterborne epoxy coating for road guardrail and preparation method of self-cleaning waterborne epoxy coating | |
CN102993903A (en) | Waterborne epoxy conductive paint and preparation method thereof | |
CN102993909A (en) | Solvent-free epoxy anticorrosive paint for ballast tank of ship and preparation method thereof | |
CN104530858A (en) | Water-based anticorrosive coating added with nanometer TiO2 | |
CN104250512A (en) | Water-based alcohol acid primer-topcoat antirust paint and preparation method thereof | |
CN104725977B (en) | Double-component aqueous epoxy zinc rich primer of heavy antisepsis and preparation method thereof | |
CN104263189A (en) | Epoxy zinc-rich primer containing phosphorus-titanium powder and preparing method thereof | |
CN104387916A (en) | Coating composition for rapidly repairing damaged skin coat of spacecraft | |
CN103709901A (en) | Nanometer solvent-free epoxy antirust paint and preparation method thereof | |
CN103333581B (en) | A kind of Nano cerium oxide/epoxy composite paint and preparation method thereof |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
C14 | Grant of patent or utility model | ||
GR01 | Patent grant |